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A novel visible light promoted formation of CAryl‐S bonds through electron donor‐acceptor (EDA) complexes of alkylamines with 5‐ and 6‐membered (hetero)arene halides is presented. This represents the first EDA‐based thiolation method not relying on π‐π or a thiolate‐anion‐π interactions and provides a facile access to heteroarene radicals, which can be suitably trapped by disulfide derivatives to...
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